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Electrochemical mass spectrometry was recently introduced for direct study of the products of electrochemical processes For this purpose, an electrochemical cell is connected to the vacuum chamber of a mass spectrometer by a porous Teflon membrane This membrane is at the electrolyte side covered by a layer of porous platinum serving as a working electrode When the pore size is suitably selected, the solvent molecules do not pass through the hydrophobic Teflon membrane, but some molecules generated at the platinum electrode (eg H2, O2, NO, NO2, CO2) can penetrate through the membrane, and are subsequently detected by the mass spectrometer The analytical response is rather fast, typically < 05 s, which allows the measurement of mass-potential curves in parallel with usual current-potential diagrams.

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With parallel polarization, the probe light sees the extraordinary refractive index of trans-azobenzene and the mean index of cis-azobenzene in the nonirradiated and radiated areas, respectively, and the difference is large; in contrast, with perpendicular polarization, the difference is between the ordinary refractive index of trans-azobenzene and the mean index of cis-azobenzene, which is much smaller The second and stable grating formed at longer exposure times is the result of a structural reorganization and rearrangement in the ATE lm under strain Though the slow dynamics is reminiscent of the formation of SRG in azobenzene polymers (Kim et al, 1995; Rochon et al, 1995), no SRG was found by AFM, which is no surprise because the used s s polarization geometry for the two recording beams is known to be ineffective for inducing SRG (Viswanathan et al.

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According to the used potential regime, we can distinguish the mass spectrometric cyclic voltammetry, MSCV (with triangular potential changes) or differential electrochemical mass spectrometryp, DEMS (with square-wave potential changes) The electrochemical mass spectrometry seems promising, especially for the study of anodic oxidation of organic substances For instance, the detection of CO2 during anodic oxidation of propylene carbonate is a suitable complementary method to SNIFTIRS (see the example discussed on page 334) Electrochemical scanning tunnelling microscopy (ESTM) has recently been recognized as a powerful technique for in-situ characterization of the topography of electrode surfaces extending to the atomic level This method was originally developed for the study of conducting surfaces in vacuum, but is readily applicable also to surfaces in gaseous or liquid environment The latter application was first demonstrated in 1986 on graphite in aqueous solutions.

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, 1999), and the con nement of azo-SCLCP in its microdomains should hinder the mass transport (Breiner et al, 2007) The different nature of the second grating is also hinted by the less important polarization dependence of the diffraction ef ciency For samples with a well-developed second grating, changing the polarization of the probe light to be perpendicular to the strain decreases Z by only B30%, in contrast with the 90% drop for the rst grating The strong index modulation remained 7 months after the recording also implies that the grating was not caused by any difference in orientation or conformation of the B8% azobenzene polymer in the ATE lm; rather it was formed through structural changes of the whole elastomer.

The principle of ESTM is very simple: it is based on electron tunnelling between the studied electrode surface and a tip of sharply pointed wire, which is placed in close vicinity above the studied surface The tunnelling current decreases exponentially with the distance of the tip from the surface (roughly by an order of magnitude for every distance increase by 01 nm) A significant tunnelling current flows therefore only between several atoms at the apex of the tip and the nearest atoms in the examined surface The exponential decay of the tunnelling current with distance enables one to measure the vertical position of the tip with a precision in the order of 001 nm By sweeping the tip across the studied surface, an image of its topography with a comparable vertical resolution can be obtained (the lateral resolution is about 02 nm).

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If azobenzene groups were the sole factor responsible for the second grating, the grating structure would disappear days after the holographic recording as a result of the thermally activated cis trans backisomerization, restoring the equilibrium concentration of trans-azobenzene throughout the whole lm What could be the structural rearrangement in a stretched ATE lm subjected to holographic recording that is responsible for the formation of the second grating On the basis of what is known about SBS, the following analysis can be proposed The ATE sample contains some 8% azobenzene polymer grafts chemically connected to the PB chains, with the azobenzene polymer forming microdomains embedded in the PB matrix In a stretched lm, in addition to the glassy PS cylindrical microdomains (Fig 117), the azo-SCLCP microdomains may also act as cross-links and support part of the extensional stress.

The experimental set-up usually utilizes a piezoelectric tripod as a support of the tip (Fig 536) This is movable vertically and laterally over the examined surface; the vertical distance is fixed by a feedback loop to a constant tunnelling current at each point of the scan The contours of the surface are thus visualized by voltage changes needed to move the piezoelectric tripod to a desired position The in-situ ESTM was utilized for studying adsorbed or underpotential-.

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